T-SDNY 001-2018 農(nóng)藥制劑中非明示農(nóng)藥成分限量

ICS65.100G25T/SDNY001-2018農(nóng)藥制劑中非明示農(nóng)藥成分限量LimitsofunrevealedPesticidesinPesticidePreparations（發(fā)布稿）2018-10-09發(fā)布 2018-11-01實施山東省農(nóng)藥行業(yè)協(xié)會發(fā)布T/SDNY001-2018T/SDNY001-2018PAGE\*ROMANPAGE\*ROMANII目次前言 II范圍 1規(guī)范性引用文件 1定義 2要求 2試驗方法 5安全提示 5一般規(guī)定 5抽樣 5定性分析方法 5定量分析方法 6檢驗結果的判定 8附錄A（資料性附錄）51種農(nóng)藥標樣的質(zhì)譜圖 8附錄B（資料性附錄）51種農(nóng)藥的保留時間、定量離子、定性離子及定量離子與定性離子的豐度比……………………………20前 言本標準有效期限五年，到期復審。本標準附錄A為資料性附錄。本標準由山東省農(nóng)藥行業(yè)協(xié)會提出。本標準主要起草單位：山東省農(nóng)藥行業(yè)協(xié)會。本標準首次發(fā)布日期：2018年10月09日。T/SDNY001-2018T/SDNY001-2018PAGEPAGE11農(nóng)藥制劑中非明示農(nóng)藥成分限量范圍本標準規(guī)定了農(nóng)藥制劑中63種非明示農(nóng)藥成分限量的要求、試驗方法。本標準適用于在農(nóng)業(yè)生產(chǎn)中經(jīng)稀釋后常量噴施的農(nóng)藥制劑。規(guī)范性引用文件GB/T334敵百蟲原藥GB/T1605商品農(nóng)藥采樣方法GB2549敵敵畏原藥GB/T6682-2008分析實驗室用水規(guī)格和試驗方法GB/T6694氰戊菊酯原藥GB/T8170-2008數(shù)值修約規(guī)則與極限數(shù)值的表示和判定GB/T9551百菌清原藥GB/T95568辛硫磷原藥GB9558晶體樂果GB/T12685三環(huán)唑原藥GB/T13649殺螟硫磷原藥GB/T19604毒死蜱原藥GB20685硫丹原藥GB/T20695高效氯氟氰菊酯原藥GB/T22172多效唑原藥GB/T22175烯唑醇原藥GB/T22602戊唑醇原藥GB22609丁硫克百威原藥GB/T22619聯(lián)苯菊酯原藥GB/T22621霜霉威原藥GB/T22623咪鮮胺原藥GB/T24749丙環(huán)唑原藥GB/T24756噻嗪酮原藥GB/T28126吡蟲啉原藥GB/T28130噠螨靈原藥GB/T28131溴氰菊酯原藥GB29384乙酰甲胺磷原藥GB/T29385GB/T33809HG2460.1五氯硝基苯原藥HG/T2206甲霜靈原藥HG/T2209噠嗪硫磷原藥HG/T2844甲氰菊酯原藥HG/T2846三唑磷原藥HG/T2850速滅威原藥HG/T2853異丙威原藥HG/T3285異稻瘟凈原藥HG/T3287馬拉硫磷原藥HG/T3293三唑酮原藥HG/T3304稻瘟靈原藥HG/T3619仲丁威原藥HG/T3625丙溴磷原藥HG/T3627氯氰菊酯原藥HG/T3629高效氯氰菊酯原藥HG/T3755啶蟲脒原藥HG/T3764腈菌唑原藥HG/T3765炔螨特原藥HG/T4460苯醚甲環(huán)唑原藥HG/T44642蟲酰肼原藥HG/T4466辛酰溴苯腈原藥HG/T4927氟氯氰菊酯原藥HG/T4928高效氟氯氰菊酯原藥HG/T4933茚蟲威原藥HG/T5126異菌脲原藥HG/T5232醚菌酯原藥HG/T5236吡唑醚菌酯原藥HG/T5239吡丙醚原藥NY/T2990-2016禁限用農(nóng)藥定性定量分析方法定義非明示農(nóng)藥成分 unrevealedPesticides農(nóng)藥產(chǎn)品中含有的除農(nóng)藥標簽、說明書、產(chǎn)品標準、登記證上標明的以外的農(nóng)藥成分。要求631表1農(nóng)藥制劑中63種非明示農(nóng)藥成分限量指標序號項目指 標1百菌清質(zhì)量分數(shù)，%≤1.02苯醚甲環(huán)唑質(zhì)量分數(shù)，%≤0.73吡丙醚質(zhì)量分數(shù)，%≤0.24吡蟲啉質(zhì)量分數(shù)，%≤1.05吡唑醚菌酯質(zhì)量分數(shù)，%≤1.0表1農(nóng)藥制劑中63種非明示農(nóng)藥成分限量指標（續(xù)）序號項 目指 標6丙環(huán)唑質(zhì)量分數(shù)，%≤0.57丙溴磷質(zhì)量分數(shù)，%≤1.08蟲酰肼質(zhì)量分數(shù)，%≤0.49噠螨靈質(zhì)量分數(shù)，%≤0.610噠嗪硫磷質(zhì)量分數(shù)，%≤0.411稻瘟靈質(zhì)量分數(shù)，%≤0.812敵百蟲質(zhì)量分數(shù)，%≤1.013敵敵畏質(zhì)量分數(shù)，%≤1.014丁硫克百威質(zhì)量分數(shù)，%≤0.115啶蟲脒質(zhì)量分數(shù)，%≤1.016毒死蜱質(zhì)量分數(shù)，%≤0.117多效唑質(zhì)量分數(shù)，%≤0.318氟蟲腈質(zhì)量分數(shù)，%≤0.119氟氯氰菊酯質(zhì)量分數(shù)，%≤0.120高效氟氯氰菊酯質(zhì)量分數(shù)，%≤0.121高效氯氟氰菊酯質(zhì)量分數(shù)，%≤0.522高效氯氰菊酯質(zhì)量分數(shù)，%≤0.223甲拌磷質(zhì)量分數(shù)，%≤0.0524甲基異柳磷質(zhì)量分數(shù)，%≤0.0125甲氰菊酯質(zhì)量分數(shù)，%≤0.426甲霜靈質(zhì)量分數(shù)，%≤0.727腈菌唑質(zhì)量分數(shù)，%≤0.828克百威質(zhì)量分數(shù)，%≤0.0229樂果質(zhì)量分數(shù)，%≤0.130聯(lián)苯菊酯質(zhì)量分數(shù)，%≤0.131硫丹質(zhì)量分數(shù)，%≤0.132氯氰菊酯質(zhì)量分數(shù)，%≤0.233馬拉硫磷質(zhì)量分數(shù)，%≤0.934咪鮮胺質(zhì)量分數(shù)，%≤0.9表1農(nóng)藥制劑中63種非明示農(nóng)藥成分限量指標(續(xù))序號項目指 標35醚菌酯質(zhì)量分數(shù)，%≤1.036嘧霉胺質(zhì)量分數(shù)，%≤0.837滅多威質(zhì)量分數(shù)，%≤0.538滅線磷質(zhì)量分數(shù)，%≤0.0539氰戊菊酯質(zhì)量分數(shù)，%≤0.140炔螨特質(zhì)量分數(shù)，%≤1.041噻蟲嗪質(zhì)量分數(shù)，%≤1.042噻嗪酮質(zhì)量分數(shù)，%≤0.543三環(huán)唑質(zhì)量分數(shù)，%≤1.044三唑磷質(zhì)量分數(shù)，%≤0.145三唑酮質(zhì)量分數(shù)，%≤0.546殺螟硫磷質(zhì)量分數(shù)，%≤1.047霜霉威質(zhì)量分數(shù)，%≤1.048水胺硫磷質(zhì)量分數(shù)，%≤0.0549速滅威質(zhì)量分數(shù)，%≤0.550涕滅威質(zhì)量分數(shù)，%≤0.1351五氯硝基苯質(zhì)量分數(shù)，%≤0.852戊唑醇質(zhì)量分數(shù)，%≤1.053烯唑醇質(zhì)量分數(shù)，%≤0.354辛硫磷質(zhì)量分數(shù)，%≤0.855辛酰溴苯腈質(zhì)量分數(shù)，%≤0.656溴氰菊酯質(zhì)量分數(shù)，%≤0.157氧樂果質(zhì)量分數(shù)，%≤0.0158乙酰甲胺磷質(zhì)量分數(shù)，%≤0.159異丙威質(zhì)量分數(shù)，%≤0.460異稻瘟凈質(zhì)量分數(shù)，%≤1.061異菌脲質(zhì)量分數(shù)，%≤1.062茚蟲威質(zhì)量分數(shù)，%≤0.663仲丁威質(zhì)量分數(shù)，%≤1.0試驗方法安全提示一般規(guī)定GB/T6682GB/T8170-20084.3.3抽樣GB/T1605200mL（液體）250g（固體）。產(chǎn)品質(zhì)量控制檢驗應在首件產(chǎn)品中抽樣。定性分析方法1212NY/T2990-20163.251方法提要試樣用丙酮溶解，用氣相色譜-質(zhì)譜儀進行檢測，通過與標準質(zhì)譜圖比對進行定性。若存在農(nóng)藥助劑干擾，可提取定性離子進行確認。試劑和溶液a）水（GB/T6682）:一級水。b）丙酮。乙腈：色譜純。農(nóng)藥標樣儲備溶液：稱取百菌清、苯醚甲環(huán)唑、吡丙醚、吡蟲啉、吡唑醚菌酯、丙環(huán)唑、丙溴磷、蟲酰肼、噠螨靈、噠嗪硫磷、稻瘟靈、敵百蟲、敵敵畏、啶蟲脒、毒死蜱、多效唑、氟氯氰菊酯、0.025g（0.0001g）50mL50mL（4℃避光條2）儀器氣相色譜-質(zhì)譜儀：具有電子轟擊電離源（EI）。30m×0.25mm（id）HP-5MS0.25μm（或同等效果的色譜柱。c）色譜工作站。微量進樣器：10μL。0.45μm。f）超聲波清洗器。氣相色譜-質(zhì)譜參考操作條件601min15℃/min2003min20℃/min280℃15min230℃。氣體流量（mL/min）：載氣（He）：1.7。c）分流比：30：1。d）進樣體積：1μL。e）電離電壓：70eV。f）離子源溫度：230g）接口溫度：280℃。h）掃描模式：全掃描。氣相色譜-質(zhì)譜測定步驟a）51種農(nóng)藥混合標樣溶液的制備5.4.2.2e)1mL25mL試樣溶液的制備0.1g（0.0001g）50mL5min，冷卻至室溫25mL測定在5.4.2.4操作條件下。待儀器基線穩(wěn)定后，按照混合標樣溶液、試樣溶液的順序進行測定。結果判定5.4.2.52.0%以內(nèi)，并且質(zhì)譜圖基本一致，則可判定試樣中含有該農(nóng)藥成分。5.4.2.52.0%以內(nèi)；并且在試樣溶液和標樣溶液色譜峰中，提取的定性離子同時出現(xiàn)、且定性離子的相對豐度一致（相對豐度>50%，允許±10%偏差；20%<相對豐度≤50%，允許±15%偏差；10%<相對豐度≤20%，允許±205.2農(nóng)藥成分時，應按5.5對其進行質(zhì)量分數(shù)的測定。（51種農(nóng)藥標樣的質(zhì)譜圖見附錄A。51種農(nóng)藥的保留時間、定量離子、定性離子及定量離子與定性離子的豐度比見附錄B。）定量分析方法1212NY/T2990-20163.35151種農(nóng)藥質(zhì)量分數(shù)的測定試驗參照表2方法進行。表251種農(nóng)藥質(zhì)量分數(shù)測定方法序號項 目測定方法1百菌清GB/T95512苯醚甲環(huán)唑HG/T44603吡丙醚HG/T52394吡蟲啉GB/T281265吡唑醚菌酯HG/T52366丙環(huán)唑GB/T247497丙溴磷HG/T36258蟲酰肼HG/T44649噠螨靈GB/T2813010噠嗪硫磷HG/T220911稻瘟靈HG/T330412敵百蟲GB/T33413敵敵畏GB254914啶蟲脒HG/T375515毒死蜱GB/T1960416多效唑GB/T2217217氟氯氰菊酯HG/T492718高效氟氯氰菊酯HG/T492819高效氯氟氰菊酯GB/T2069520高效氯氰菊酯HG/T362921甲氰菊酯HG/T284422甲霜靈HG/T220623腈菌唑HG/T376424聯(lián)苯菊酯GB/T2261925氯氰菊酯HG/T362726馬拉硫磷HG/T3287表251種農(nóng)藥質(zhì)量分數(shù)測定方法（續(xù)）序號項 目測定方法27咪鮮胺GB/T2262328醚菌酯HG/T523229嘧霉胺GB/T2938530氰戊菊酯GB/T669431炔螨特HG/T376532噻蟲嗪GB/T3380933噻嗪酮GB/T2475634三環(huán)唑GB/T1268535三唑磷HG/T284636三唑酮HG/T329337殺螟硫磷GB/T1364938霜霉威GB/T2262139速滅威HG/T285040五氯硝基苯HG2460.141戊唑醇GB/T2260242烯唑醇GB/T2217543辛硫磷GB/T955644辛酰溴苯腈HG/T446645溴氰菊酯GB/T2813146異丙威HG/T285347異稻瘟凈HG/T328548異菌脲HG/T512649茚蟲威HG/T493350仲丁威HG/T361951硫丹GB20685附 錄 A（資料性附錄）51種農(nóng)藥標樣的質(zhì)譜圖51種農(nóng)藥標樣的質(zhì)譜圖見圖A.1~A.51。2661226612283547628698109 12413515916819422927021910075502500.0 25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0A.1百菌清標樣質(zhì)譜圖

m/z323265323265505575100111133140173202209327230253288298345100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 m/z圖A.2苯醚甲環(huán)唑標樣質(zhì)譜圖1367813678965167115157186197226321100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 m/zA.3吡丙醚標樣質(zhì)譜圖211126211126994428569012814015637311426151168176182194100755025025.0

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m/zA.4吡蟲啉標樣質(zhì)譜圖132164132164516377111141179194325285357100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 m/z圖A.5吡唑醚菌酯標樣質(zhì)譜圖691736917325912814519119355828696109159100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 m/zA.6丙環(huán)唑標樣質(zhì)譜圖139431394320897339271256316726929775189232159 251311329374376100755025073207732072211332787710534135551116178295161235253313369 387399100

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0m/zA.7丙溴磷標樣質(zhì)譜圖755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0A.8蟲酰肼標樣質(zhì)譜圖147117147117579113210555165309364187217273100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 m/zA.9噠螨靈標樣質(zhì)譜圖779777976512519910920447137 1531713402352492671007550250100

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m/z圖A.11稻瘟靈標樣質(zhì)譜圖10979109791394731951122214563127151169185192259100755025025.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 m/zA.12敵百蟲標樣質(zhì)譜圖1097910979471852960659397145128155174220100755025025.0

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200.0 m/zA.13敵敵畏標樣質(zhì)譜圖152561525612615316667221909973112139187207194 277100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 m/zA.14啶蟲脒標樣質(zhì)譜圖T/SDNY001-2018Inten.T/SDNY001-2018Inten.PAGEPAGE131979719797314258125286651692154493134161244276318351755025050.0

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325.0 350.0m/zA.15毒死蜱標樣質(zhì)譜圖2361252361258216757127417011289140153179193206218278100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 m/zA.16多效唑標樣質(zhì)譜圖163165163165206226779151127109228261 283294 315333356397433100755025050 100

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250 300 350 400 m/z氟氯氰菊酯標樣質(zhì)譜圖163165163165206226779112751109228261283294 315333356397433100755025050.0 75.0

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175.0200.0225.0250.0275.0300.0325.0350.0375.0400.0425.0m/zA.18高效氟氯氰菊酯標樣質(zhì)譜圖181197181197141775115291115225241 262286 314325349449404414100755025050 100 150 200 250 300 350 400 450m/zA.19高效氯氟氰菊酯標樣質(zhì)譜圖163181163181915112741152208109225243265 284315379400415755025050.0

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275.0 300.0 325.0 350.0m/z圖A.21甲氰菊酯標樣質(zhì)譜圖452064520613214616059771056519219022023424991120174279100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 m/z圖A.22甲霜靈標樣質(zhì)譜圖179821798215055206125 1371632452887089101115219100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 m/z圖A.23腈菌唑標樣質(zhì)譜圖181165181165446389101115152197225281322 341422100755025050 100

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200 250 300 350 400 m/z圖A.24聯(lián)苯菊酯標樣質(zhì)譜圖T/SDNY001-2018T/SDNY001-2018PAGEPAGE22163181163181915112741152208109225243265 284315379400415100755025050 100

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250 300 350 400 m/z圖A.25氯氰菊酯標樣質(zhì)譜圖29125291259317315847637914331111184211205238256284100755025025.0 50.0

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75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0圖A.27咪鮮胺標樣質(zhì)譜圖

325.0 350.0 375.0m/z1161311161312065989771462234151162175254282313100755025050.0 75.0 100.0

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225.0 250.0 275.0 300.0 m/z19842198425165778291100107118134 143157169184196100755025050.0 75.0 100.0 125.0 150.0 175.0 m/z圖A.29嘧霉胺標樣質(zhì)譜圖125167125167152181225419775511520989100755025050.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 m/z圖A.30氰戊菊酯標樣質(zhì)譜圖135811358139173691072011829117158215231252267350295323335100755025025.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 m/z圖A.31炔螨特標樣質(zhì)譜圖圖A.32噻蟲嗪分解物標樣質(zhì)譜圖1057710577577041172100119140157190194216230249263 277290305100755025050.0

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60 70 80 90 100 110 120 130 140 150 160 170 180圖A.38霜霉威標樣質(zhì)譜圖

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350 400 m/z圖A.51硫丹標樣質(zhì)譜圖附 錄 B（資料性附錄）51種農(nóng)藥的保留時間、定量離子、定性離子及定量離子與定性離子的豐度比51種農(nóng)藥的保留時間、定量離子、定性離子及定量離子與定性離子的豐度比見表B.1。表B.151種農(nóng)藥的保留時間、定量離子、定性離子及定量離子與定性離子的豐度比序號項目保留時間定量離子定性離子定性離子1百菌清12.1266（100）264（72）268（40）2苯醚甲環(huán)唑-123.7323（100）265（95）325（67）苯醚甲環(huán)唑-223.9323（100）265（101）325（66）3吡丙醚95737-68-119.6136（100）226（7）186（2）4吡蟲啉16.399（100）126（87）211(132)5吡唑醚菌酯20.3132（100）164（35）325（4）6丙環(huán)唑-117.7259（100）175（54）261（65）丙環(huán)唑-217.8259（100）175（60）261（64）7丙溴磷16.7339（100）337（98）374（41）8蟲酰肼23.4105（100）133（192）296（3）9噠螨靈20.1147（100）148（12）309（4）10噠嗪硫磷30.1340（100）199（400）188（350）11稻瘟靈25.8290（100）118（238）204（83）稻瘟靈-d425.8294（100）235（85）193（150）12敵百蟲8.879（100）109 (130)145 (54)13敵敵畏7.2109（100）185（34）220（7）14丁硫克百威17.9160（100）118（69）323（16）15啶蟲脒18.2152（100）126（77）166（42）16毒死蜱15.0314（100）316（75）286（53）17多效唑16.2236（100）125（80）238（31）18氟氯氰菊酯21.5206（100）199（65）226（77）19高效氟氯氰菊酯21.591（100）163（526）206（279）20高效氯氟氰菊酯19.7181（100）197（100）141（20）21高效氯氰菊酯22.3/22.491（100）163（161）181（148）表B.151種農(nóng)藥的保留時間、定量